CN102236274B - A method for producing a toner and an erasable toner - Google Patents
A method for producing a toner and an erasable toner Download PDFInfo
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- CN102236274B CN102236274B CN201110102695.0A CN201110102695A CN102236274B CN 102236274 B CN102236274 B CN 102236274B CN 201110102695 A CN201110102695 A CN 201110102695A CN 102236274 B CN102236274 B CN 102236274B
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
- G03G9/00—Developers
- G03G9/08—Developers with toner particles
- G03G9/0802—Preparation methods
- G03G9/0804—Preparation methods whereby the components are brought together in a liquid dispersing medium
- G03G9/0806—Preparation methods whereby the components are brought together in a liquid dispersing medium whereby chemical synthesis of at least one of the toner components takes place
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
- G03G9/00—Developers
- G03G9/08—Developers with toner particles
- G03G9/087—Binders for toner particles
- G03G9/08742—Binders for toner particles comprising macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- G03G9/08755—Polyesters
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
- G03G9/00—Developers
- G03G9/08—Developers with toner particles
- G03G9/09—Colouring agents for toner particles
- G03G9/0928—Compounds capable to generate colouring agents by chemical reaction
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Abstract
The invention relates to a method for producing a toner and an erasable toner. There is provided a method for producing a toner that includes encapsulated erasable colored fine particles aggregated with fine particles that contain at least a binder resin and a release agent. The method includes: mixing a dispersion of erasable fine particles with an aggregating agent to form an aggregating agent-containing colored fine particle dispersion; and mixing the aggregating agent-containing colored fine particle dispersion with a fine particle dispersion that contains at least a binder resin and a release agent, so as to aggregate the aggregating agent-containing colored fine particles with the fine particles that contain at least a binder resin and a release agent. In this way, the encapsulated colored fine particles are prevented from being released from the resultant toner particles, and an erasable toner can be obtained that has a narrow particle size distribution and that produces less fogging.
Description
The cross reference of related application
The application based on and require the U.S. Provisional Patent Application No.61/328 that submitted on April 27th, 2010,378 right of priority and rights and interests, and its full content is hereby expressly incorporated by reference.
Technical field
Present embodiment relates to toner, particularly can eliminate the manufacture method of toner and the toner of so making.
Background technology
As can eliminate toner, known according to No. 7,354,885, U.S. Patent No. for example have a toner that contains colour generation compound and developer and can eliminate by heating.In this technology, by mixing comminuting method, colour generation compound and developer are dissolved together with adhesive resin mixing, to enter toner inside.As for this toner, by can make the colour killing of lettering part in about 1 hour to 3 hours to the paper after lettering heating under 100 ℃ to 200 ℃, and then, can recycle the paper after colour killing.Reduce the consumption of paper, thereby can contribute to reducing carrying capacity of environment.
Yet, in the situation that use mixing comminuting method, owing to being mixing to the high temperature of 200 ℃ of left and right and the high shear force at 100 ℃, leuco dye and developer evenly spread in adhesive resin, hinder the reaction of leuco dye (colour generation compound) and developer, the colour developing concentration that toner occurs descends.In addition, have colour killing at toner materials such as adhesive resin or release agents and do the used time, the same colour developing concentration that toner occurs reduces when mixing, so need to select the little material of colour killing effect as the toner material.Particularly, about adhesive resin, there is following shortcoming (problem points): can only use the such specific resin that does not have the colour killing effect of styrene-butadiene class, and the vibrin of fixation performance excellence, styrene acrylic resin use very difficult because easily affecting the colour killing effect.
Therefore, as the manufacture method beyond mixing comminuting method, the present inventor has studied by aggegation in aqueous medium merges the eliminable painted wet type method for making (US2010/209839A1) that obtains toner with particulates such as particulate and adhesive resins.According to the method, because being generates microparticle agglutination, thus can small particle diameter, can utilize the condition of the heat treated that makes its fusion to become shape spherical from potato-like.In addition, need not to experience the mechanical shearing or the high thermal process that dissolve in mixing, just can eliminate the conglomerate integrations such as particulate and adhesive resin.For example, so long as surpass the temperature of the Tg of binder resin, namely can less than the ratio lower temperature of 80 ℃ realize toner.Therefore, paintedly reversibly eliminate fully with particulate and by heating process is non-about encapsulated the elimination, the method is effective method for making.
Yet, in the situation that encapsulated this can be eliminated particulate, find that the dispersion stabilization of this particulate is very high, this particulate is difficult to enter in toner fully.Hence one can see that, and the fine powder of toner increases, image degradation.
Summary of the invention
embodiments of the present invention provide a kind of toner method for making, the method is made toner by making by the toner eliminated after encapsulated and the microparticle agglutination that contains at least adhesive resin and release agent, wherein, at first, mixing can be eliminated toner dispersion liquid and agglutinant, formation contains the toner dispersion liquid of agglutinant, then, mix and describedly contain the toner dispersion liquid of agglutinant and contain at least the particle dispersion liquid of adhesive resin and release agent, make the toner that contains agglutinant and contain at least the microparticle agglutination of adhesive resin and release agent.
Description of drawings
Fig. 1 is the process flow diagram of making according to the toner of one embodiment of the invention.
Embodiment
The present invention can make and improved the problems referred to above and prevented from being broken away from and the toner of generation fine powder from toner by the toner eliminated after encapsulated.
According to an embodiment of the present invention, agglutinant is played a role, make by the dispersion stabilization of the toner eliminated after encapsulated and reduce, then mix with other compositions that contain adhesive resin, and make its aggegation, thereby produce toner.
Below, describe for embodiments of the present invention.In following record, if no special instructions, expression composition " part " and " % " is weight basis.
According to an embodiment of the present invention, it is the method for being made toner by the toner eliminated after encapsulated and the microparticle agglutination that contains at least adhesive resin and release agent by making, wherein, at first, mixing can be eliminated toner dispersion liquid and agglutinant, formation contains the toner dispersion liquid of agglutinant, then, mix and describedly contain the toner dispersion liquid of agglutinant and contain the particle dispersion liquid of adhesive resin and release agent at least, make the toner that contains agglutinant and contain at least the microparticle agglutination of adhesive resin and release agent.According to the method, by improving by the compendency of the toner after encapsulated and reduce the dispersion stabilization of each particle, thereby can will stably be joined in toner by the toner after encapsulated.
Fig. 1 illustrates the manufacturing flow chart in an embodiment more specifically.
At first, obtain by the dispersion liquid of the toner eliminated after encapsulated, and with itself and agglutinant aqueous solution, obtain containing the painted dispersion liquid of agglutinant.
Encapsulatedly eliminated toner, namely contained at least leuco dye, developer, depigmenting agent by the nucleus of the toner eliminated after encapsulated.If it is better that depigmenting agent has temperature hysteresis.Can obtain the toner of moment elimination by this composition.
Leuco dye is can be by the supplied for electronic compound of developer color development.For example, can list diphenyl-methane phthalide-type, Phenylindole phthalide-type, indoles phthalide-type, diphenyl-methane diazobenzene phthaleins, Phenylindole diazobenzene phthaleins, Material of Fluoran, styryl quinolines, two diazonium rhodamine lactone etc.These compounds can mix use more than 2 kinds.
The developer that uses in the present invention is to give the electrophilic compound of proton to leuco dye.for example have: phenols, the metal phenolate salt, carboxylic acid metal's salt, aromatic carboxylic acid and carbon number are 2～5 aliphatic carboxylic acid, benzophenone, sulphonic acids, sulfonate, the phosphoric acid class, the phosphate metal salt, the acid phosphoric acid ester class, the acid phosphoric acid ester metallic salt, the phosphorous acid class, the phosphorous acid metallic salt, single phenols, Polyphenols, 1, 2, 3-triazole and derivant thereof etc., can also list as its substituting group and have alkyl, aryl, acyl group, alkoxy carbonyl group, carboxyl and ester thereof or amide group, the compound of halogen etc. and bis-phenol, triphenol etc., phenol formaldehyde condensation resins etc. also have their metallic salt.These compounds can mix use more than 2 kinds.
With respect to 1 part of leuco dye, preferably use developer with the ratio of 0.5 part～10 parts, particularly 1 part～5 parts.If 0.5 part of less than, color development concentration step-down, if surpass 10 parts, be difficult to make its complete colour killing.
As the depigmenting agent that uses in the present invention, get final product so long as can hinder the color reaction of leuco dye and developer and become colourless depigmenting agent by heating in 3 composition systems of leuco dye (colour generation compound), developer, depigmenting agent, can use known depigmenting agent.
The moment elimination property of the depigmenting agent of the color development colour killing mechanism that can form the temperature hysteresis of utilizing depigmenting agent that discloses in JP60-264285A, JP2005-1369A, JP2008-280523A especially, is excellent.In case more than the potpourri of 3 one-tenth subsystems of color development has been heated to specific colour killing temperature T h with this, can make its colour killing.And, even the temperature that the potpourri after colour killing is cooled to below Th also can be kept the colour killing state.When further reducing temperature, below specific secondary color temperature T c, the color reaction of leuco dye and developer brings back to life again, and the reversible color development colour killing reaction that what is called turns back to the color development state can occur.Especially, if room temperature is Tr, the depigmenting agent that uses in the present invention preferably satisfies the relation of Th＞Tr＞Tc.
Can cause the depigmenting agent of this temperature hysteresis, alcohols, ester class, ketone, ethers, amide-type are for example arranged.
Preferred ester class.specifically can list: the carboxylate that contains the substituted aromatic ring, contain the carboxylic acid that has or not the substituted aromatic ring and the ester of aliphatic alcohol, the carboxylate that contains cyclohexyl in molecule, fatty acid with without the ester of substituted aromatic alcohol or phenol, the ester of fatty acid and branching aliphatic alcohol, the ester of dicarboxylic acids and aromatic alcohols or branching aliphatic alcohol, the cinnamic acid dibenzyl ester, the stearic acid heptyl ester, didecyl adipate, the hexane diacid dilaurate, hexane diacid two myristinates, hexane diacid two (cetyl) ester, the hexane diacid distearate, trilaurin, myristin, glyceryl tristearate, glycerine two myristinates, distearin etc.These esters can mix use more than 2 kinds.
With respect to 1 part of leuco dye, preferably use these depigmenting agents with the ratio of 1 part～500 parts, particularly 4 parts～99 parts.If 1 part of less than is difficult to occur complete colour killing state, surpass 500 parts if use, color development concentration may descend.
The encapsulated method of nucleus that is used for the colorant particles of encapsulated 3 compositions that contain above-mentioned leuco dye, developer and depigmenting agent has in surface aggregate method, coacervation, situ aggregation method, intra-liquid desiccation method, liquid sclerosis by embrane method (orifice method) etc.
Particularly preferably use with melamine resin as the situ aggregation method of shell component, with urethane resin with as the surface aggregate method of shell component etc.
During situ aggregation method, at first, dissolving mixes above-mentioned 3 compositions, makes its emulsification in water soluble polymer or water phase surfactant mixture.Then, add melamino-formaldehyde prepolymer aqueous solution, and heated polymerizable, thereby realize encapsulated.
During the surface aggregate method, dissolving mixes above-mentioned 3 compositions and polyisocyanic acid prepolymer, makes its emulsification in water soluble polymer or water phase surfactant mixture body.Then, add the polyacid bases such as diamines or glycol, and heated polymerizable, thereby realize encapsulated.
Like this, the volume average particle size that obtains being measured by laser method is 0.5 μ m～3.5 μ m, be preferably the aqueous dispersions of the encapsulated toner of 1.0 μ m～3.0 μ m and size-grade distribution distinctness.Like this, by carrying out encapsulated 3 compositions of the leuco dye (colour generation compound) that consists of toner, developer, depigmenting agent that make and closely coexist in capsule eliminating toner, and adhesive resin is also deposited intervention wherein, so formed the color development the changed-colour killing system of can completing rapidly between the high color development state of concentration and colour killing state.
In the situation that toner comprises the depigmenting agent with temperature hysteresis, usually, toner is colourless under this state, as required, after reclaiming from aqueous dispersions, is cooled to below secondary color temperature T c, becomes colored state, then carries out subsequent processing.
Then, again encapsulated toner and surfactant are distributed in water together as required, add agglutinant according to the present invention in this aqueous dispersions, obtain containing the toner dispersion liquid of agglutinant.Solid portion (encapsulated toner) concentration in the aqueous dispersion liquid of this moment is preferably 10%～50%, is particularly preferably 20%～30%.When adding agglutinant, but being heated to 50 ℃ to 70 ℃ limits with aqueous dispersions, the limit adds agglutinant.Due to very high by the dispersion stabilization of the toner after encapsulated, therefore can use the strong agglutinant of cohesive force.As the example of preferred agglutinant, can exemplify the above slaine of divalent.As concrete example, can use the 3 valency slaines such as the divalent slaines such as magnesium chloride, lime chloride, magnesium sulphate, calcium nitrate, zinc chloride, iron protochloride, ferrous sulphate and aluminium sulphate, aluminum chloride.With respect to 1 part of toner, preferably use agglutinant with the ratio of 0.01 part～1 part, particularly 0.1 part～0.7 part.In addition, in the situation that use identical agglutinant, preferably setting agglutinant is agglutinant with respect to more than 2 times of relative quantity of the toner composition (namely by the aggegation composition) in the mixing material that contains the toner dispersion liquid of agglutinant and the particle dispersion liquid that contains at least adhesive resin, release agent described later with respect to the relative quantity of the toner in the toner dispersion liquid that contains coagulator, thereby effectively reduces the dispersion stabilization of encapsulated toner.In addition, as required, also can reclaim encapsulated toner or remove the aqueous dispersion liquid phase and carry out Separation of Solid and Liquid the aqueous dispersions after agglutinant adds processing, remove unnecessary agglutinant.Add agglutinant and be for reduce in the future in the potpourri with other toner compositions such as adhesive resin by the free property (dispersion stabilization) of the toner after encapsulated.Therefore, needn't require toner aggegation in containing the toner dispersion liquid of agglutinant.
Then, mixing this contains the painted dispersion liquid of agglutinant and contains adhesive resin and the particulate of release agent.
As binder resin, use the existing resins of using bonding agent as toner such as the phenylethylene resin series such as vibrin, polystyrene, Styrene-Butadiene, styrene-propene multipolymer.The glass transition temperature of preferred adhesive resin is that 40 ℃～80 ℃, softening point are 80 ℃～180 ℃, separately or be generally the fixing temperature of 50 ℃～200 ℃, preferred 50 ℃～150 ℃ as required and together with the following release agent of use.As adhesive resin, the good vibrin of fixation performance particularly preferably.In addition, the acid value of vibrin can be more than 1 (mg KOH/g).By having acid value, can bring into play the effect of the alkaline pH adjusting agent in micronize, obtain the chromonic particles of small particle diameter.
As release agent, can be according to adjusting the purposes such as fixing temperature, release property, use such as with the oxide of fat hydrocarbon wax, fat hydrocarbon wax or their segmented copolymer, vegetable wax, mineral wax, fatty acid ester as the wax class of major component etc.
With the calculation of total of adhesive resin and release agent, preferably used adhesive resin and release agent by the toner after encapsulated with the ratio of 1 part～99 parts, particularly 2 parts～19 parts to every 1 part.
Also can add charge control agents such as containing metal azo-compound, containing metal salicylic acid derivative compound in the particulate take adhesive resin as major component as required.
In order to form the particulate that contains above-mentioned adhesive resin, release agent, charge control agent etc., can dissolve mix these compositions and pulverize as required after, utilize by nozzle to spue and the method for carrying out putting down in writing the US2010/209839A1 (its content is hereby expressly incorporated by reference) such as method, emulsion polymerization method of microminiaturization is carried out from high-pressure pump.
Although be not the particulate take these adhesive resins as major component directly can not be dropped in the above-mentioned toner dispersion liquid that contains agglutinant to mix, but after preferably making separately it be distributed in the waterborne liquid that contains surfactant, then mix with the toner dispersion liquid that contains agglutinant.
When this mixes, add as required and append agglutinant, and make the mutual aggegation of these particulates.As the agglutinant that appends that adds herein, contain in the toner dispersion liquid of agglutinant the equally preferably slaine more than the use divalent of institute's agglutinant that uses with formation, but and do not require it is slaine of the same race.As the aggegation dosage that is present in the dispersion liquid system that produces by mixing, with respect to 1 part of toner composition, preferably with 0.001 part to 0.5 part, particularly the ratio of 0.01 part to 0.2 part is used.
Preferably, the temperature of the dispersion liquid system in aggegation is 25 ℃～80 ℃ left and right, and adding as required after polycarboxylate sodium's aqueous solution etc. merges stabilization agent, preferably under agitation make at leisure temperature rise to the glass transition temperature of adhesive resin～100 ℃ of left and right, promote the fusion of agglutination particle.
Then, particle is merged in washing, dry aggegation, by adding the additives such as silicon dioxide that particle diameter is 10nm～100nm left and right or titanium dioxide, obtain according to (use limited diameter under the mensuration in 100 μ m apertures: the volume mean diameter of the particle diameter distribution of 2.0 μ m) trying to achieve is that 4 μ m～15 μ m, 50% number mean diameter are the toner of 4 μ m～15 μ m with Ku Ertefa.Narrow diameter distribution according to the feature of the toner of the inventive method manufacturing, show as: free less due to fine powder, so the mean diameter of 50% number is near volume average particle size, variation coefficient CV (mean diameter of=standard deviation/50% number) little to be below 40%, preferred little of being below 35%.
Embodiment below is shown.
The preparation of＜colored particles dispersion liquid 〉
heat dissolving by as the 3-(2-ethoxy 4-diethylamino phenyl) of leuco dye-1 part of 3-(1-Ethyl-2-Methyl indol-3-yl)-4-azepine phthalide (3-(2-ェ ト キ シ-4-ジ ェ チ Le ァ ミ ノ Off ェ ニ Le)-3-(1-ェ チ Le-2-メ チ Le ィ Application De one Le-3-ィ Le)-4-ァ ザ Off タ リ De), as 2 of developer, 5 parts of two (4-hydroxy phenyl) HFC-236fa of 2-, composition as 50 parts of compositions of diester compound of the heptandioic acid of depigmenting agent and 2-(4-benzyloxy phenyl) ethanol, with this dissolved matter and 20 parts of aromatic series polyisocyanic acid prepolymers (many value of aromatic series ィ ソ シ ァ ネ one ト プ レ Port リ マ one) that are mixed with as capsule agent, the solution that ethyl acetate is 40 parts is put in 250 part of 8% polyvinyl alcohol water solution, emulsion dispersion is also continuing stir about after 1 hour under 70 ℃, interpolation is as 2 parts of the water-soluble modified fatty amines (the water-soluble fatty sex change ァ ミ of family Application) of reactant, and liquid temperature is remained on 90 ℃ of also lasting stir abouts 3 hours, obtain colourless capsule particle.Then, this capsule particle dispersion put into the freezer of-20 ℃ and made its color development, obtaining the colored particles dispersion liquid of the blueness of solid portion concentration 24%.Utilize the laser method particle footpath measure of spread device (SALD7000 processed of Shimadzu Seisakusho Ltd.; Measure particle size range 10nm～300 μ m) measure this colored particles, its volume average particle size is 2 μ m.In addition, colour killing temperature T h is 79 ℃ fully, and color development temperature T c is-10 ℃ fully.
＜contain the preparation of the particle dispersion liquid of adhesive resin and release agent 〉
To carry out even mixing in dry mixer as 1 part of vibrin 94 portions of (45 ℃ of glass transition temperatures, 100 ℃ of softening points), cured 5 parts of release agent rice, the charge control agent hodogaya chemical commercial production (TN-105) of adhesive resin, then, carried out melting mixing with twin shaft mixing roll pond shellfish ironworker manufacturing PCM-45 under 80 ℃.With needle mill, resulting toner composition is pulverized in order to cross 2mm and sieved, then with the BANTAM muller, it is ground into mean grain size 50 μ m.
Then, 0.45 part of 0.9 part of surfactant neopelex, pH adjusting agent dimethylamino-ethanol (ジ メ チ Le ァ ミ ノ ェ タ ノ one Le) is mixed with 68.65 parts of ion exchange waters, and 30 parts of the crushed materials of toner composition have been scattered in this aqueous solution, carry out vacuum defoamation, obtained dispersion liquid.
next, use the NANO3000 (U.S. grain company make) of following setting: will be immersed in 12m heat interchange in oil bath with high press fit pipe as the heating part, the high press fit pipe of the nozzle of will contain multi pack 0.13 μ m and 0.28 μ m is as pressurization part, with multi pack have 0.4 a μ m, 1.0 μ m, 0.75 μ m, 1.5 μ m, 1.0 the middle press fit pipe in the pond (cell) in μ m aperture is as relief portion, can be by water-cooled 12m heat interchange pipe arrangement from the beginning as cooling end, and at 180 ℃, under 150MPa, dispersion liquid has been carried out the micronize processing, and keep 180 ℃ on one side, reduce pressure on one side, then, be cooled to 30 ℃, obtained containing the dispersion liquid of adhesive resin and release agent.Utilize above-mentioned laser method particle footpath measure of spread device (SALD7000) to measure resulting particle, its volume average particle size is 0.5 μ m.
＜embodiment 1 〉
70 parts of colored particles dispersion liquids obtained above are heated to 60 ℃, and the limit is stirred the limit with homogenizer (IKA company produce) with 6500rpm and is slowly added 30 parts of 25% aluminum sulfate aqueous solutions.Placed 1 hour after adding, and after being cooled to room temperature, obtain containing the colored particles dispersion liquid of agglutinant.With Ku Ertefa particle size distribution analyzer (the many particle size analyzers 3 of Ku Erte society; (particle size range: 2.0 μ m～60 μ m) measure the particle footpath, obtaining 50% volume mean diameter Dv is 2.8 μ m in 100 μ m apertures.
Then, mix this 2 parts of colored particles dispersion liquid that contain agglutinant, 15 parts of particle dispersion liquids that contain adhesive resin and release agent, 83 parts of ion exchange waters, the limit is stirred the limit with homogenizer (IKA company system) with 6500rpm and is added 5 parts of aluminum sulfate aqueous solution 5% aqueous solution, then, the limit is stirred the limit with 800rpm and is warming up to 40 ℃ in being provided with the 1L tank diameter of blade.After placing 1 hour under 40 ℃, 10 parts of polycarboxylate sodium's aqueous solution of interpolation 10% are heated to 68 ℃, place after 1 hour, and are cooling, and obtain blue toner dispersion liquid.
Then, this toner dispersion liquid is repeatedly filtered and adopts the washing of ion exchange water, wash become 50 μ S/cm to the conductivity of filtrate till.Afterwards, being dried to water percentage with vacuum drier is below 1.0% by weight, and obtains drying particulate.
After drying, with respect to 100 parts of drying particulates, as 0.5 part of the titanium dioxide of 2 parts of the hydrophobic silicas of adjuvant stuff and other stuff footpath 30nm, particle footpath 20nm, make it be attached to the drying particulate surface, but obtain the colour killing toner.With above-mentioned Ku Ertefa particle size distribution analyzer mensuration particle footpath, obtaining 50% number mean diameter Dp is 8.2 μ m.In addition, variation coefficient CV (standard deviation/50% number mean diameter Dp) is 32%, is high-definition size-grade distribution.
The ferrite carrier that mixes resulting toner and covered by organic siliconresin carries out image output with Toshiba's Tag MFP processed (e-studio 4520c) under the environment of 25 ℃/50%RH, obtain not having the image of photographic fog.Then, be that 70 ℃, paper transfer rate are adjusted into 30mm/sec with the fuser Temperature Setting, obtain the chromophore image of image color 0.5.In addition, for to non-image confirmation toner photographic fog, measure the image color of non-image section, its concentration is 0.05, and is identical with the image color of blank sheet of paper.
Be 100 ℃ with the fuser Temperature Setting and transmit the chromophore image obtain with paper transfer rate 100mm/sec, thereby confirm that image becomes colorless.
Image Saving after colour killing in the freezer of-20 ℃, is confirmed to return to colour killing image color 0.5 in the past.
＜comparative example 1 〉
Mix 1.5 parts of above-mentioned colored particles dispersion liquids, contain 15 parts of particle dispersion liquids, 83 parts of the ion exchange waters of above-mentioned adhesive resin and release agent, stir after the limit adds 5 parts of aluminum sulfate aqueous solution 5% aqueous solution with 6500rpm with homogenizer (IKA company produce) on the limit, and the limit is stirred the limit with the 1L tank diameter that is provided with blade with 800rpm and is warming up to 40 ℃.After placing 1 hour under 40 ℃, add 10 parts of polycarboxylate sodium's aqueous solution of 10% and be heated to 68 ℃, place after 1 hour, cooling, obtain blue toner dispersion liquid.
Then, this toner dispersion liquid is repeatedly filtered and adopts the washing of ion exchange water, wash become 50 μ S/cm to the conductivity of filtrate till.Afterwards, being dried to water percentage with vacuum drier is below 1.0% by weight, and obtains drying particulate.
After drying, with respect to 100 parts of drying particulates, as adjuvant mix with embodiment 1 in 2 parts of identical hydrophobic silicas, 0.5 part of the titanium dioxide of use, make it be attached to the drying particulate surface, thereby but obtain the colour killing toner.In the same manner with Ku Ertefa particle size distribution analyzer mensuration particle footpath, its 50% number mean diameter Dp is 7.5 μ m with embodiment 1.In addition, CV (standard deviation/50% number mean diameter Dp) is 53%, is the size-grade distribution of the many broadnesses of fine powder.
Is mixed by the ferrite carrier that organic siliconresin covers in the same manner with the toner that obtains with embodiment 1, carry out image with Toshiba's Tag MFP processed (e-studio4520c) and export, non-image generation toner is fuzzy.Then, setting the fuser temperature is 70 ℃, and adjusting the paper transfer rate is 30mm/sec, obtains the chromophore image of image color 0.5.In addition, for confirming the toner photographic fog of non-image section, measure the image color of non-image section, its concentration is 0.15, than image color 0.05 height of blank sheet of paper.
Claims (8)
1. a toner manufacturing method, make toner by making by the toner eliminated after encapsulated and the microparticle agglutination that contains at least adhesive resin and release agent, wherein,
At first, mixing can be eliminated toner dispersion liquid and agglutinant, formation contains the toner the eliminated dispersion liquid of agglutinant, then, mix and describedly contain the toner the eliminated dispersion liquid of agglutinant and contain the particle dispersion liquid of adhesive resin and release agent at least, make the toner eliminated that contains agglutinant and contain at least the microparticle agglutination of adhesive resin and release agent.
2. toner manufacturing method according to claim 1, wherein,
Agglutinant is the above slaine of divalent.
3. toner manufacturing method according to claim 1, wherein,
The agglutinant that interpolation is appended in the mixed liquor of the toner the eliminated dispersion liquid that contains agglutinant and the particle dispersion liquid that contains at least adhesive resin and release agent.
4. toner manufacturing method according to claim 1, wherein,
Containing agglutinant in the toner the eliminated dispersion liquid of agglutinant is to contain in the mixed liquor of the toner the eliminated dispersion liquid of agglutinant and the particle dispersion liquid that contains at least adhesive resin and release agent agglutinant with respect to eliminating quality relative quantity 2 times or more of toner with the total amount of the particulate that contains at least adhesive resin and release agent with respect to the quality relative quantity that can eliminate toner.
5. toner manufacturing method according to claim 3, wherein,
Containing agglutinant in the toner the eliminated dispersion liquid of agglutinant is to contain in the mixed liquor of the toner the eliminated dispersion liquid of agglutinant and the particle dispersion liquid that contains at least adhesive resin and release agent agglutinant with respect to eliminating quality relative quantity 2 times or more of toner with the total amount of the particulate that contains at least adhesive resin and release agent with respect to the quality relative quantity that can eliminate toner.
6. toner manufacturing method according to claim 1, wherein,
Comprised leuco dye, developer and depigmenting agent by the nucleus of the toner eliminated after encapsulated.
7. toner manufacturing method according to claim 6, wherein,
Depigmenting agent is to eliminating that toner is given under the colour killing temperature T h higher than room temperature Tr colour killing and the depigmenting agent with temperature hysteresis of the characteristic of color development again at the temperature lower than room temperature Tr.
8. can eliminate toner for one kind, toner manufacturing method according to claim 1 and making, described eliminate toner comprise by encapsulated and processed by agglutinant after the toner eliminated and with described by encapsulated and processed by agglutinant after the particulate that contains at least adhesive resin and release agent of the toner eliminated aggegation
Described eliminate toner definite particle diameter variation coefficient is below 40% by the mean grain size of standard deviation/50% number.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US32837810P | 2010-04-27 | 2010-04-27 | |
| US61/328,378 | 2010-04-27 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102236274A CN102236274A (en) | 2011-11-09 |
| CN102236274B true CN102236274B (en) | 2013-06-12 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110102695.0A Expired - Fee Related CN102236274B (en) | 2010-04-27 | 2011-04-22 | A method for producing a toner and an erasable toner |
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|---|---|
| US (1) | US8603722B2 (en) |
| JP (1) | JP5584648B2 (en) |
| CN (1) | CN102236274B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5586552B2 (en) * | 2010-12-07 | 2014-09-10 | 株式会社東芝 | Method for producing electrophotographic developer |
| JP5431423B2 (en) * | 2011-07-08 | 2014-03-05 | 東芝テック株式会社 | Decolorizable toner and method for producing the same |
| JP5955788B2 (en) * | 2013-01-17 | 2016-07-20 | 東芝テック株式会社 | Erasable toner |
| WO2018110200A1 (en) | 2016-12-14 | 2018-06-21 | 株式会社日立製作所 | Temperature detection material, temperature detection ink using same, temperature indicator, method for manufacturing temperature detection material, and product management system |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1243274A (en) * | 1998-01-23 | 2000-02-02 | 株式会社东芝 | Method for eliminating image-forming material |
| CN101017339A (en) * | 2006-02-10 | 2007-08-15 | 施乐公司 | Toner composition |
| CN101046651A (en) * | 2006-03-28 | 2007-10-03 | 富士施乐株式会社 | Image forming apparatus, image forming method and toner |
| JP2007256359A (en) * | 2006-03-20 | 2007-10-04 | Fuji Xerox Co Ltd | Image forming apparatus and method |
| CN101144994A (en) * | 2006-09-11 | 2008-03-19 | 花王株式会社 | Method for manufacturing toner for electrophotography |
Family Cites Families (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3474780B2 (en) * | 1998-08-04 | 2003-12-08 | 株式会社東芝 | Erasable image forming material |
| JP2000330321A (en) * | 1999-05-21 | 2000-11-30 | Pilot Ink Co Ltd | Temperature sensitive discolorable dry toner |
| US20070020554A1 (en) * | 2005-07-25 | 2007-01-25 | Xerox Corporation | Toner process |
| JP4825472B2 (en) * | 2005-09-01 | 2011-11-30 | 花王株式会社 | Toner for electrophotography |
| JP2008015333A (en) * | 2006-07-07 | 2008-01-24 | Fuji Xerox Co Ltd | Toner for electrostatic image development, and electrostatic image developer and image forming method using the same |
| JP5006682B2 (en) * | 2007-04-06 | 2012-08-22 | 花王株式会社 | Toner for electrophotography |
| JP2009300991A (en) * | 2008-05-14 | 2009-12-24 | Pilot Ink Co Ltd | Thermochromic color-memory toner, cartridge storing the same, image forming apparatus, cartridge set and image forming apparatus set |
| CN101807018B (en) * | 2009-02-16 | 2013-10-16 | 东芝泰格有限公司 | Developing agent and method for producing the same |
| EP2431444B1 (en) * | 2009-05-12 | 2019-11-13 | The Pilot Ink Co., Ltd. | Thermochromic color-memory composition, and thermochromic color-memory microcapsule pigment having the composition encapsulated therein |
| JP5396651B2 (en) * | 2009-11-13 | 2014-01-22 | パイロットインキ株式会社 | Temperature-sensitive color change color memory toner and cartridge containing the same, image forming apparatus, cartridge set, and image forming apparatus set |
| EP2341394B1 (en) * | 2010-01-04 | 2016-08-31 | Toshiba TEC Kabushiki Kaisha | Toner |
-
2011
- 2011-04-14 US US13/086,661 patent/US8603722B2/en not_active Expired - Fee Related
- 2011-04-19 JP JP2011093192A patent/JP5584648B2/en active Active
- 2011-04-22 CN CN201110102695.0A patent/CN102236274B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1243274A (en) * | 1998-01-23 | 2000-02-02 | 株式会社东芝 | Method for eliminating image-forming material |
| CN101017339A (en) * | 2006-02-10 | 2007-08-15 | 施乐公司 | Toner composition |
| JP2007256359A (en) * | 2006-03-20 | 2007-10-04 | Fuji Xerox Co Ltd | Image forming apparatus and method |
| CN101046651A (en) * | 2006-03-28 | 2007-10-03 | 富士施乐株式会社 | Image forming apparatus, image forming method and toner |
| CN101144994A (en) * | 2006-09-11 | 2008-03-19 | 花王株式会社 | Method for manufacturing toner for electrophotography |
Also Published As
| Publication number | Publication date |
|---|---|
| US20110262850A1 (en) | 2011-10-27 |
| US8603722B2 (en) | 2013-12-10 |
| JP2011232750A (en) | 2011-11-17 |
| JP5584648B2 (en) | 2014-09-03 |
| CN102236274A (en) | 2011-11-09 |
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